ASTM E775-87(1996)
(Test Method)Standard Test Methods for Total Sulfur in the Analysis Sample of Refuse-Derived Fuel
Standard Test Methods for Total Sulfur in the Analysis Sample of Refuse-Derived Fuel
SCOPE
1.1 These test methods cover two alternative procedures for the determination of total sulfur in prepared analysis samples of solid forms of refuse-derived fuel (RDF). Sulfur is included in the ultimate analysis of RDF.
1.2 The test methods appear in the following order: Test Sections Eschka Method 8 to 11 Bomb Washing Method 12 to 13
1.3 These test methods may be applicable to any waste material from which a laboratory analysis sample can be prepared.
1.4 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are for information only.
1.5 This standard may involve hazardous materials, operations, and equipment. This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific precautionary statements see Section 6.
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Designation: E 775 – 87 (Reapproved 1996)
Standard Test Methods for
Total Sulfur in the Analysis Sample of Refuse-Derived Fuel
This standard is issued under the fixed designation E 775; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3.1.1 refuse-derived fuels—solid forms of refuse-derived
fuels from which appropriate analytical samples may be
1.1 These test methods cover two alternative procedures for
prepared are defined as follows in ASTM STP 832:
the determination of total sulfur in prepared analysis samples
RDF-1—Wastes used as a fuel in as-discarded form with
of solid forms of refuse-derived fuel (RDF). Sulfur is included
only bulky wastes removed.
in the ultimate analysis of RDF.
RDF-2—Wastes processed to coarse particle size with or
1.2 The test methods appear in the following order:
without ferrous metal separation.
Test Sections
RDF-3—Combustible waste fraction processed to particle
Eschka Method 8-11
Bomb Washing Method 12 and 13
sizes, 95 % passing 2-in. square screening.
RDF-4—Combustible waste fraction processed into powder
1.3 These test methods may be applicable to any waste
form, 95 % passing 10-mesh screening.
material from which a laboratory analysis sample can be
RDF-5—Combustible waste fraction densified (compressed)
prepared.
into the form of pellets, slugs, cubettes, or briquettes.
1.4 The values stated in inch-pound units are to be regarded
as standard. The values given in parentheses are for informa-
4. Summary of Test Methods
tion only.
4.1 Eschka Method— A weighed sample and Eschka mix-
1.5 This standard does not purport to address all of the
ture are ignited together and the sulfur is precipitated from the
safety concerns, if any, associated with its use. It is the
resulting solution as barium sulfate (BaSO ). The precipitate is
responsibility of the user of this standard to establish appro- 4
filtered, ashed, and weighed.
priate safety and health practices and determine the applica-
4.2 Bomb Washing Method—Sulfur is precipitated as
bility of regulatory limitations prior to use. For specific
BaSO from the oxygen-bomb calorimeter washings and the
precautionary statements see Section 6.
precipitate is filtered, ashed, and weighed.
2. Referenced Documents
5. Significance and Use
2.1 ASTM Standards:
2 5.1 The standards are available to producers and users of
D 1193 Specification for Reagent Water
RDF for determining the total sulfur content of the fuel.
E 180 Practice for Determining the Precision of ASTM
Methods for Analysis and Testing of Industrial Chemicals
6. Precautions
E 711 Test Method for Gross Calorific Value of Refuse-
6.1 Due to the origins of RDF in municipal waste, common
Derived Fuel by the Bomb Calorimeter
sense dictates that some precautions should be observed when
E 829 Practice for Preparing Refuse-Derived Fuels (RDF)
conducting tests on the samples. Recommended hygienic
Laboratory Samples for Analysis
practices include use of gloves when handling RDF; wearing
3. Terminology dust masks (NIOSH-approved type), especially while milling
RDF samples; conducting tests under negative pressure hood
3.1 Definitions of Term Specific to This Standard:
when possible; and washing hands before eating or smoking.
These test methods are under the jurisdiction of ASTM Committee D34 on
Waste Management and is the direct responsibility of Subcommittee D34.06 on
Recovery and Reuse.
Current edition approved Aug. 28, 1987. Published October 1987. Originally
published as E 775 – 81. Last previous edition E 775 – 81.
Annual Book of ASTM Standards, Vol 11.01.
3 5
Annual Book of ASTM Standards, Vol 15.05. Thesaurus on Resource Recovery Terminology, ASTM STP 832, ASTM, 1983,
Annual Book of ASTM Standards, Vol 11.04. p.72.
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E 775
7. Sampling 9.8 Methyl Orange Indicator Solution (0.2 g/L)—Dissolve
0.2 g of methyl orange in 1000 mL of hot water and filter.
7.1 RDF products are frequently nonhomogeneous. For this
9.9 Sodium Carbonate (saturated solution)—Dissolve ap-
reason significant care should be exercised to obtain a repre-
proximately 60 g of crystallized sodium carbonate
sentative laboratory sample from the RDF lot to be character-
(Na CO ·10H O) or 20 g of anhydrous sodium carbonate
ized.
2 3 2
(Na CO ) in 100 mL of water, using a sufficient excess of
7.2 The sampling method for this procedure should be based 2 3
Na CO to ensure a saturated solution.
on agreement between the involved parties.
2 3
9.10 Sodium Hydroxide Solution (100 g/L)—Dissolve 100 g
7.3 The laboratory sample must be air-dried and particle
of sodium hydroxide (NaOH) in 1 L of water. This solution
size reduced to pass a 0.5-mm screen as described in Practice
may be used in place of Na CO solution.
E 829. This procedure must be performed carefully to preserve
2 3
the sample’s representative characteristics (other than particle
10. Procedure
size) while preparing the analysis sample to be used in the
procedures.
10.1 Preparation of Sample and Eschka Mixture—Weigh to
the nearest 0.1 mg about1gof mixed air-dried analysis sample
TEST METHOD A—ESCHKA METHOD
and3gof Eschka mixture on glazed paper. Mix thoroughly.
The amount of sample to be taken will depend on the amount
8. Apparatus
of BaCl solution required (see 10.3.5 and Note 2).
8.1 Gas (Note 1) or Electric Muffle Furnace or Burners, for
10.1.1 Quantitatively transfer the mixture to a porcelain
igniting the sample with Eschka mixture and for igniting the
capsule or porcelain crucible or platinum crucible, and cover
barium sulfate (BaSO ).
with about1gof Eschka mixture.
NOTE 1—Gas may contain sulfur compounds in sufficient quantities to
10.2 Ignition—Heat the crucible over a gas flame as de-
affect the results.
scribed in 10.2.1, or in a gas- or electrically heated muffle
8.2 Crucibles or Capsules—Porcelain capsules, ⁄8 in. (22
furnace as described in 10.2.2. The use of artificial gas for
mm) in depth and 1 ⁄4 in. (44 mm) in diameter, or porcelain
heating the sample and Eschka mixture is permissible only
crucibles of 30-mL capacity, high or low-form, or platinum
when the crucibles are heated in a muffle (see Note 2).
crucibles of similar size shall be used for igniting the sample
10.2.1 Heat the crucible, placed in a slanting position
with the Eschka mixture. Porcelain, platinum, Alundum, or
partially covered on a triangle, over a very low flame. This
silica crucibles of 10 to 15-mL capacity shall be used for the
prevents rapid expulsion of the volatile matter and affords more
final ignition step (see 10.3.8).
complete oxidation of the sulfur. After 30 min of low flame
heating, gradually increase the temperature and occasionally
9. Reagents
stir the mixture until all black particles have disappeared,
9.1 Purity of Reagents—Reagent grade chemicals shall be
which is an indication of complete combustion.
used in all tests. Unless otherwise indicated, it is intended that
10.2.2 Place the crucible in a cold muffle furnace and
all reagents shall conform to the specifications of the American
gradually raise the temperature to 800 6 25°C in about 1 h.
Chemical Society, where such specifications are available.
Maintain this maximum temperature until upon stirring all
Other grades may be used, provided it is first ascertained that
black particles have disappeared (about 1 ⁄2 h).
the reagent is of sufficiently high purity to permit its use
10.3 Subsequent Treatment:
without lessening the accuracy of the determination.
10.3.1 Remove the crucible, cool, and empty the contents
9.2 Purity of Water— Unless otherwise indicated, refer-
quantitatively into a 200-mL beaker. Digest with 100 mL of hot
ences to water shall be understood to mean reagent water, Type
1 3
water for ⁄2 to ⁄4 h with occasional stirring.
III conforming to Specification D 1193.
10.3.2 Decant the supernatant liquid through a filter into a
9.3 Barium Chloride Solution (100 g/L)—Dissolve 100 g of
600-mL beaker. Wash the insoluble matter with hot water
barium chloride (BaCl ·2H O) and dilute to 1 L with water.
2 2
several times using 25 mL of water at each washing and filter
9.4 Bromine Water (saturated)—Add an excess of bromine
the washings through the filter paper into the 600-mL beaker.
to 1 L of water.
After washing, transfer the insoluble matter to the filter and
9.5 Eschka Mixture— Thoroughly mix 2 parts by weight of
wash five times with hot water, keeping the mixture well
light calcined magnesium oxide (MgO) with 1 part of anhy-
agitated, collecting the wash waters in the 600-mL beaker.
drous sodium carbonate (Na CO ). Both materials should be as
2 3
10.3.3 Treat the filtrate with 10 to 20 mL of saturated
free as possible from sulfur.
bromine water. Make slightly acid with HCl and boil to expel
9.6 Hydrochloric Acid (1 + 1)—Mix equal volumes of con-
the liberated bromine.
centrated HCl (sp gr 1.19) and water.
10.3.4 Neutralize using methyl orange indicator with NaOH
9.7 Hydrochloric Acid (1 + 9)
...
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